CN111572022B - Method for improving degradation performance of L-polylactic acid bone scaffold by using kaolinite - Google Patents
Method for improving degradation performance of L-polylactic acid bone scaffold by using kaolinite Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
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- B29C64/153—Processes of additive manufacturing using only solid materials using layers of powder being selectively joined, e.g. by selective laser sintering or melting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a method for improving degradation performance of a levorotatory polylactic acid bone scaffold by using kaolinite, which comprises the following steps: (1) dispersing KL powder and PLLA powder into absolute ethyl alcohol to respectively obtain KL suspension and PLLA suspension; (2) mixing the KL suspension and the PLLA suspension to obtain a KL/PLLA mixed suspension, and filtering and drying to obtain KL/PLLA composite powder; (3) and selectively sintering the KL/PLLA composite powder by using laser to obtain the KL/PLLA composite bone scaffold. The PLLA molecular chains are rearranged by laser sintering, the KL sheet is introduced, the KL sheet is used as a nucleation site in a PLLA matrix, the PLLA molecular chains are crystallized on the KL sheet, and the crystals grow out of order along different directions due to the disordered arrangement of the KL sheet in the PLLA matrix, so that the integral crystallinity of the PLLA is reduced, and the degradation rate of the PLLA scaffold is accelerated.
Description
Technical Field
The invention belongs to the technical field of degradable high-molecular bone scaffolds, and relates to a method for improving the degradation performance of a levorotatory polylactic acid bone scaffold by using kaolinite.
Background
The levorotatory polylactic acid (PLLA) is a well-recognized biomaterial, and has good biocompatibility and degradability. In the human body, the lactic acid can be firstly degraded into lactic acid, then further decomposed into carbon dioxide and water, and finally discharged out of the body by metabolism without generating any harmful residues. In addition, the elastic modulus of PLLA is close to that of human bone tissue, so that the stress shielding effect of materials such as metal and ceramic caused by overlarge modulus can be avoided. However, the degradation rate of PLLA in human physiological environment is too slow, the time of 2-3 years is required for complete degradation, and it is difficult to match with the regeneration rate of bone tissue (the regeneration time of new bone is 12-18 weeks) to hinder the growth of new bone tissue, which severely limits the application of PLLA in bone tissue engineering.
Kaolinite (KL) is widely distributed, is mainly formed by aluminosilicate minerals such as feldspar and common pyroxene in the weathering process, is a layered silicate ceramic material, has large surface area and excellent mechanical property, and can be used as a reinforcing phase to improve the mechanical property of a polymer bone scaffold.
However, at present, no report on the use of kaolinite modified L-polylactic acid for preparing a composite bone scaffold for simultaneously improving the mechanical property and the degradation property of the composite bone scaffold exists.
Disclosure of Invention
In order to solve the problem that the degradation rate of the conventional PLLA bone scaffold is too slow and is difficult to match with the regeneration rate of bone tissues so as to hinder the growth of new bone tissues, the invention aims to provide a method for improving the degradation performance of a L-polylactic acid bone scaffold by using kaolinite.
In order to achieve the technical purpose, the invention adopts the following technical scheme
A method for improving degradation performance of a levorotatory polylactic acid bone scaffold by using kaolinite comprises the following steps:
(1) dispersing KL powder and PLLA powder into absolute ethyl alcohol to respectively obtain KL suspension and PLLA suspension;
(2) mixing the KL suspension and the PLLA suspension to obtain a KL/PLLA mixed suspension, and filtering and drying to obtain KL/PLLA composite powder;
(3) and selectively sintering the KL/PLLA composite powder by using laser to obtain the KL/PLLA composite bone scaffold.
In a preferable scheme, the particle size of the KL powder is 10-30 mu m, and the purity is not lower than 99%.
Preferably, the particle size of the PLLA powder is 1-10 mu m, and the purity is not lower than 99%.
Preferably, the mass ratio of the KL powder to the PLLA powder is 2.5: 97.5-7.5: 92.5. the inventors found that when the KL content is too low, the accelerated PLLA bone scaffold degradation rate is not significant; when the KL is too much, the KL is unevenly dispersed in the PLLA matrix, and a continuous phase is locally formed, so that the bone scaffold is unevenly melted and degraded, and the mechanical property of the bone scaffold is reduced.
In a preferable scheme, ultrasonic dispersion and magnetic stirring are adopted for the dispersion in the step (1) and the mixing in the step (2), and the ultrasonic dispersion time is 30-60 min; the magnetic stirring time is 30-60 min, and the speed is 100-500 r/min.
According to the preferable scheme, the KL/PLLA composite powder is placed in a selective laser sintering system, layer-by-layer sintering is carried out according to a preset three-dimensional model, and after sintering is finished, the unsintered powder is removed by using compressed air, so that the KL/PLLA composite bone scaffold is obtained.
In a preferred scheme, the process parameters of the selective laser sintering are as follows: the laser power is 1.5-2.5W, the scanning speed is 50-150 mm/s, the scanning interval is 0.6-1.0 mm, and the spot diameter is 1.0-1.8 mm.
The invention adopts KL to modify PLLA, and obtains the KL/PLLA composite bone scaffold by selective laser sintering. KL is a sheet-like structure, and in the selective laser sintering process, KL can be regarded as a nucleation site in a PLLA matrix, and a molecular chain of PLLA is crystallized along the KL sheet. Since the KL sheets are randomly and freely arranged in the matrix, crystals also grow in different directions, disordering the ordered arrangement of the PLLA molecular chains, which reduces the crystallinity of the PLLA molecular chains as a whole. Meanwhile, as the degradation of the polymer is started from the non-crystalline region, the crystallinity is reduced, which means that the non-crystalline region is increased, thereby accelerating the degradation of the PLLA.
Compared with the prior art, the invention has the beneficial effects that:
(1) the PLLA molecular chains are rearranged by laser sintering, the KL sheet is introduced and is used as a nucleation site in a PLLA matrix, the PLLA molecular chains are crystallized on the KL sheet, and the crystals grow out of order along different directions due to the disordered arrangement of the KL sheet in the PLLA matrix, so that the integral crystallinity of the PLLA is reduced, and the degradation rate of the PLLA scaffold is accelerated.
(2) The KL is mainly formed by aluminosilicate minerals such as feldspar and common pyroxene in the weathering process, is wide in distribution, has large surface area and excellent mechanical property, and can be used as a reinforcing phase to improve the mechanical property of the PLLA bone scaffold while improving the degradation rate of the PLLA bone scaffold.
Drawings
FIG. 1 is a graph showing the dispersion state of KL in a PLLA matrix in the KL/PLLA composite bone scaffolds prepared in examples 1-3 and the surface state of the PLLA bone scaffold prepared in comparative example 1;
FIG. 2 is a graph showing the mass loss of KL/PLLA composite bone scaffolds prepared in examples 1-3 and PLLA bone scaffolds prepared in comparative example 1 after soaking in simulated body fluid for 28 days;
FIG. 3 is a graph showing the surface topography of KL/PLLA composite bone scaffolds prepared in examples 1-3 and PLLA bone scaffolds prepared in comparative example 1 after soaking in simulated body fluid for 28 days.
Detailed Description
The following further describes embodiments of the present invention with reference to specific examples, but the present invention is not limited thereto.
Example 1
(1) Weighing 0.05g of KL powder, adding the KL powder into 100ml of absolute ethyl alcohol, performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly dispersed KL suspension;
(2) weighing 0.95g of PLLA powder, adding the PLLA powder into 100ml of absolute ethyl alcohol, performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly dispersed PLLA suspension;
(3) mixing the KL suspension liquid obtained in the step (1) and the PLLA suspension liquid obtained in the step (2), performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly mixed KL/PLLA mixed suspension liquid;
(4) pouring the KL/PLLA mixed suspension into a filtering device for standing, placing the obtained filtrate in a drying box, and drying for 24 hours to obtain KL/PLLA composite powder;
(5) placing the KL/PLLA composite powder in a laser sintering forming system, and sintering layer by layer according to a preset three-dimensional model, wherein the sintering process parameters are as follows: the laser power is 1.8W, the scanning speed is 70mm/min, the scanning distance is 0.8mm, the spot diameter is 1.5mm, after sintering is finished, the unsintered powder is removed by using compressed air, and the KL/PLLA composite bone scaffold with the KL content of 5 wt% is obtained and is marked as 5 wt% KL/PLLA.
The mechanical property test shows that the compressive strength of the 5 wt% KL/PLLA prepared in the embodiment is 45.7 MPa.
Example 2
(1) Weighing 0.025g of KL powder, adding the KL powder into 100ml of absolute ethyl alcohol, performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly dispersed KL suspension;
(2) weighing 0.975g of PLLA powder, adding the PLLA powder into 100ml of absolute ethyl alcohol, performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly dispersed PLLA suspension;
(3) mixing the KL suspension liquid obtained in the step (1) and the PLLA suspension liquid obtained in the step (2), performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly mixed KL/PLLA mixed suspension liquid;
(4) pouring the KL/PLLA mixed suspension into a filtering device for standing, placing the obtained filtrate in a drying box, and drying for 24 hours to obtain KL/PLLA composite powder;
(5) placing the KL/PLLA composite powder in a laser sintering forming system, and sintering layer by layer according to a preset three-dimensional model, wherein the sintering process parameters are as follows: the laser power is 1.8W, the scanning speed is 70mm/min, the scanning distance is 0.8mm, the diameter of a light spot is 1.5mm, after sintering is finished, unsintered powder is removed by using compressed air, and the KL/PLLA composite bone scaffold with the KL content of 2.5 wt% is obtained and is marked as 2.5 wt% KL/PLLA.
The mechanical property test shows that the compressive strength of the 2.5 wt% KL/PLLA prepared in the example is 36.1 MPa.
Example 3
(1) Weighing 0.075g of KL powder, adding the KL powder into 100ml of absolute ethyl alcohol, performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly dispersed KL suspension;
(2) weighing 0.925g of PLLA powder, adding the PLLA powder into 100ml of absolute ethyl alcohol, performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly dispersed PLLA suspension;
(3) mixing the KL suspension liquid obtained in the step (1) and the PLLA suspension liquid obtained in the step (2), performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly mixed KL/PLLA mixed suspension liquid;
(4) pouring the KL/PLLA mixed suspension into a filtering device for standing, placing the obtained filtrate in a drying box, and drying for 24 hours to obtain KL/PLLA composite powder;
(5) placing the KL/PLLA composite powder in a laser sintering forming system, and sintering layer by layer according to a preset three-dimensional model, wherein the sintering process parameters are as follows: the laser power is 1.8W, the scanning speed is 70mm/min, the scanning distance is 0.8mm, the diameter of a light spot is 1.5mm, after sintering is finished, unsintered powder is removed by using compressed air, and the KL/PLLA composite bone scaffold with the KL content of 7.5 wt% is obtained and is marked as 7.5 wt% KL/PLLA.
The mechanical property test shows that the compressive strength of the 7.5 wt% KL/PLLA prepared in the example is 40.8 MPa.
Comparative example 1
(1) Weighing 1g of PLLA powder, placing the PLLA powder in a laser sintering forming system, and sintering layer by layer according to a preset three-dimensional model, wherein the sintering process parameters are as follows: the laser power is 1.8W, the scanning speed is 70mm/min, the scanning interval is 0.8mm, the spot diameter is 1.5mm, and after sintering, the unsintered powder is removed by using compressed air to obtain a PLLA bone scaffold, which is marked as 0% KL/PLLA.
The mechanical property test shows that the compression strength of the PLLA bone scaffold prepared by the comparative example is 19.4 MPa.
FIG. 1 shows the dispersion state of KL in the PLLA matrix in the KL/PLLA composite bone scaffolds prepared in examples 1-3, and it can be seen that KL is uniformly dispersed in the PLLA matrix; while the PLLA bone scaffold prepared in comparative example 1 had a relatively flat surface.
FIG. 2 shows the mass loss of the KL/PLLA composite bone scaffolds prepared in examples 1-3 and the PLLA bone scaffold prepared in comparative example 1 after soaking in a simulated body fluid for 28 days, wherein the mass loss of the PLLA bone scaffold alone is 1.9%; the mass loss of the KL/PLLA composite bone scaffold prepared in example 1 was 8.4%, the mass loss of the KL/PLLA composite bone scaffold prepared in example 2 was 3.8%, and the mass loss of the KL/PLLA composite bone scaffold prepared in example 3 was 12.6%.
FIG. 3 shows the surface morphology of the KL/PLLA composite bone scaffolds prepared in examples 1-3 and the PLLA bone scaffold prepared in comparative example 1 after being soaked in simulated body fluid for 28 days, and it can be seen that the surface of the pure PLLA bone scaffold has almost no pores and poor degradation performance; and with the increase of the KL content in the KL/PLLA composite bone scaffold, the surface holes are sequentially increased, and the degradation performance is sequentially improved.
Comparative example 2
(1) Weighing 0.01g of KL powder, adding the KL powder into 100ml of absolute ethyl alcohol, performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly dispersed KL suspension;
(2) weighing 0.99g of PLLA powder, adding the PLLA powder into 100ml of absolute ethyl alcohol, performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly dispersed PLLA suspension;
(3) mixing the KL suspension liquid obtained in the step (1) and the PLLA suspension liquid obtained in the step (2), performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly mixed KL/PLLA mixed suspension liquid;
(4) pouring the KL/PLLA mixed suspension into a filtering device for standing, placing the obtained filtrate in a drying box, and drying for 24 hours to obtain KL/PLLA composite powder;
(5) placing the KL/PLLA composite powder in a laser sintering forming system, and sintering layer by layer according to a preset three-dimensional model, wherein the sintering process parameters are as follows: the laser power is 1.8W, the scanning speed is 70mm/min, the scanning distance is 0.8mm, the diameter of a light spot is 1.5mm, after sintering is finished, non-sintered powder is removed by using compressed air, and the KL/PLLA composite bone scaffold with the KL content of 1 wt% is obtained and is marked as 1 wt% KL/PLLA.
The mechanical property test shows that the compressive strength of the 1 wt% KL/PLLA prepared in the example is 25.3 MPa.
Comparative example 3
(1) Weighing 0.1g of KL powder, adding the KL powder into 100ml of absolute ethyl alcohol, performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly dispersed KL suspension;
(2) weighing 0.9g of PLLA powder, adding the PLLA powder into 100ml of absolute ethyl alcohol, performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly dispersed PLLA suspension;
(3) mixing the KL suspension liquid obtained in the step (1) and the PLLA suspension liquid obtained in the step (2), performing ultrasonic dispersion for 30min at room temperature, and performing magnetic stirring for 30min at the speed of 300r/min to obtain a uniformly mixed KL/PLLA mixed suspension liquid;
(4) pouring the KL/PLLA mixed suspension into a filtering device for standing, placing the obtained filtrate in a drying box, and drying for 24 hours to obtain KL/PLLA composite powder;
(5) placing the KL/PLLA composite powder in a laser sintering forming system, and sintering layer by layer according to a preset three-dimensional model, wherein the sintering process parameters are as follows: the laser power is 1.8W, the scanning speed is 70mm/min, the scanning distance is 0.8mm, the spot diameter is 1.5mm, after sintering is finished, the unsintered powder is removed by using compressed air, and the KL/PLLA composite bone scaffold with the KL content of 10 wt% is obtained and is marked as 10 wt% KL/PLLA.
The mechanical property test shows that the compressive strength of the 10 wt% KL/PLLA prepared in the example is 37.4 MPa.
Claims (7)
1. A method for improving the degradation performance of a levorotatory polylactic acid bone scaffold by using kaolinite is characterized by comprising the following steps:
(1) dispersing KL powder and PLLA powder into absolute ethyl alcohol to respectively obtain KL suspension and PLLA suspension;
(2) mixing the KL suspension and the PLLA suspension to obtain a KL/PLLA mixed suspension, and filtering and drying to obtain KL/PLLA composite powder;
(3) and selectively sintering the KL/PLLA composite powder by using laser to obtain the KL/PLLA composite bone scaffold.
2. The method for improving the degradation performance of the L-polylactic acid bone scaffold by using the kaolinite according to claim 1, wherein the method comprises the following steps: the particle size of the KL powder is 10-30 mu m, and the purity is not lower than 99%.
3. The method for improving the degradation performance of the L-polylactic acid bone scaffold by using the kaolinite according to claim 1, wherein the method comprises the following steps: the particle size of the PLLA powder is 1-10 mu m, and the purity is not lower than 99%.
4. The method for improving the degradation performance of the L-polylactic acid bone scaffold by using the kaolinite according to claim 1, wherein the method comprises the following steps: the mass ratio of the KL powder to the PLLA powder is 2.5: 97.5-7.5: 92.5.
5. the method for improving the degradation performance of the L-polylactic acid bone scaffold by using the kaolinite according to claim 1, wherein the method comprises the following steps: the dispersion in the step (1) and the mixing in the step (2) both adopt an ultrasonic dispersion and magnetic stirring mode, and the ultrasonic dispersion time is 30-60 min; the magnetic stirring time is 30-60 min, and the speed is 100-500 r/min.
6. The method for improving the degradation performance of the L-polylactic acid bone scaffold by using the kaolinite according to claim 1, wherein the method comprises the following steps: placing the KL/PLLA composite powder in a selective laser sintering system, sintering layer by layer according to a preset three-dimensional model, and removing unsintered powder by using compressed air after sintering is finished to obtain the KL/PLLA composite bone scaffold.
7. The method for improving the degradation performance of the L-polylactic acid bone scaffold by using the kaolinite according to claim 6, wherein the method comprises the following steps: the technological parameters of the selective laser sintering are as follows: the laser power is 1.5-2.5W, the scanning speed is 50-150 mm/s, the scanning interval is 0.6-1.0 mm, and the spot diameter is 1.0-1.8 mm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018046269A1 (en) * | 2016-09-08 | 2018-03-15 | Karl Leibinger Medizintechnik Gmbh & Co. Kg | Method for producing an implant using a calcium carbonate-containing composite powder comprising microstructured particles |
| CN108943700A (en) * | 2018-07-18 | 2018-12-07 | 中南大学 | A kind of preparation method of Poly L-lactic acid/ferroso-ferric oxide Composite Bone bracket |
| CN110538350A (en) * | 2019-09-20 | 2019-12-06 | 江西理工大学 | PLLA/ZIF-8 composite bone scaffold and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018046269A1 (en) * | 2016-09-08 | 2018-03-15 | Karl Leibinger Medizintechnik Gmbh & Co. Kg | Method for producing an implant using a calcium carbonate-containing composite powder comprising microstructured particles |
| CN108943700A (en) * | 2018-07-18 | 2018-12-07 | 中南大学 | A kind of preparation method of Poly L-lactic acid/ferroso-ferric oxide Composite Bone bracket |
| CN110538350A (en) * | 2019-09-20 | 2019-12-06 | 江西理工大学 | PLLA/ZIF-8 composite bone scaffold and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 高岭石/有机插层复合物的制备、性能及应用研究;夏华;《中国博士学位论文全文数据库》;20070215(第2期);第B014-1页 * |
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